Spectrasol Applications
Sample Type: Portland Cement
|
 Preparation: |
Weigh 0.1 gm sample into 60 mls Teflon digestion vessel. Add 2
mls water + 0.5 ml HNO3 + 3 mls HF + 7mls HCl. Place the capped
vessel in a hot water bath at 95ºC for 10 minutes. Cool, open
vessel and transfer contents to a pre-tared plastic bottle. Add
50mls Spectrasol CFA-B reagent + 50mls Spectrasol CFA-C reagent.
Dilute final solution weight to 250 gms with water.
|
| Results: |
Comparison of ICP results (n = 4) using Spectrasol Coal Fly Ash
(CFA) reagent for the NIST 633 Portland cement SRM. |
|
| Analyte |
ICP Analysis |
NIST Certified |
Recovery |
|
(%) |
(%) |
(%) |
|
| SiO3 |
2.02±0.12 |
21.8 |
101 |
| Al2O3 |
3.58±0.23 |
3.7 |
97 |
| TiO2 |
0.23±0.01 |
0.24 |
96 |
| Fe2O3 |
4.22±0.21 |
4.20 |
100 |
| CaO |
64.16±0.17 |
64.5 |
99 |
| MgO |
0.98±0.08 |
1.00 |
98 |
| Na2O |
0.66±0.03 |
0.64 |
103 |
|
| Discussion: |
The Spectrasol CFA-B reagent redissolves fluoride precipitates
such as CaF2. The CFA-C reagent deactivates free fluoride and neutralizes
the pH. The avoidance of fusions reduces the dissolved solids
in solution allowing for the use of a glass concentric nebulizer.
|
| Reference: |
Tatro, M.E., V.M. Giampa and R.J. Collins. Recent advances in the dissolution
of zeolites and coal ash for Flame AA and ICP analysis. Spectroscopy, 4,2,18 (1989). |